Effervescent composition and method of making an effervescent composition including a viscous component

ABSTRACT

Disclosed is an effervescent composition that includes a viscous component is in the form of a free flowing granulation, a tablet made from the free flowing granulation, and a method of using the effervescent composition.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a divisional of U.S. patent application Ser. No.10/963,222 filed on Oct. 12, 2004, now U.S. Pat. No. 7,507,396, whichclaims the benefit of U.S. Provisional Application No. 60/512,173, filedOct. 17, 2003, both of which are incorporated herein.

BACKGROUND

The invention relates to incorporating a viscous component in aneffervescent composition.

Viscous materials are difficult to formulate into a homogeneouseffervescent composition that is easy to handle and package. Inparticular, viscous materials can cause aggregation, which impairs theformation of a free flowing effervescent powder. Viscous materials alsostick to the equipment that is used to process effervescent compositionsincluding the tablet presses that are used to mass-produce tablets.Attempts to form tablets from compositions that include viscous agentscan produce deformed tablets that lack structural integrity.

SUMMARY

In one aspect, the invention features a method of making an effervescentcomposition, the method including heating a viscous component to atemperature of at least 45° C., the viscous component exhibiting aviscosity greater than 50,000 cps at 23° C. and 1 sec⁻¹ and a viscosityless than 5000 cps at a temperature of at least 38° C. and 1 sec⁻¹,heating a composition including an effervescent agent to a temperatureof at least 45° C., and combining the heated viscous component and theheated composition. In one embodiment, the viscous component is selectedfrom the group consisting of honey, molasses, wax and combinationsthereof. In other embodiments, the viscous component includes hopextract. In another embodiment, the viscous component includes kava.

In one embodiment, the effervescent composition includes from 5% byweight to 30% by weight of the viscous component. In another embodiment,the effervescent composition includes from about 5% by weight to about25% by weight of the viscous component. In other embodiments, theeffervescent composition includes from about 10% by weight to about 20%by weight the viscous component.

In some embodiments, the effervescent composition further includes aflow agent. In one embodiment, the flow agent is selected from the groupconsisting of silica, fumed silica, precipitated silica, magnesiumoxide, calcium phosphate, magnesium carbonate, calcium silicate, sodiumalumino silicate, and combinations thereof.

In other embodiments, the effervescent composition includes from 3% byweight to 20% by weight silica, or even from 5% by weight to 15% byweight silica.

In another aspect, the invention features a method of making a freeflowing powder that includes an effervescent composition disclosedherein.

In other aspects, the invention features a method of making aneffervescent tablet, the method including making an effervescentcomposition, and tableting the effervescent composition. In oneembodiment, the tableting includes forming a tablet having a hardness offrom 3 Kp to 15 Kp. In other embodiments, the tablet includes from 5% byweight to 30% by weight of the viscous component. In some embodiments,the tablet includes from about 10% by weight to about 20% by weight ofthe viscous component.

In another embodiment, the tablet further includes binder and lubricant.

In one embodiment, the method of making an effervescent composition,includes heating a viscous component having a viscosity greater than50,000 cps at 23° C. to a temperature sufficient to cause the componentto exhibit a viscosity no greater than 5000 cps, heating a compositionincluding an effervescent agent to a temperature of at least 45° C., andcombining the component and the heated effervescent agent to form aneffervescent composition.

In another aspect, the invention features an effervescent compositionthat includes a viscous component exhibiting a viscosity greater than50,000 cps at 23° C. and 1 sec⁻¹ and no greater than 5000 cps at atemperature of at least 38° C. and 1 sec⁻¹, effervescent agent, andsilica, the effervescent composition being a uniform, free-flowinggranulation. In some embodiments, the effervescent composition includesfrom 3% by weight to 20% by weight silica.

In another embodiment, the effervescent composition includes a viscouscomponent exhibiting a viscosity greater than 50,000 cps at 1 sec⁻¹ and23° C. and a viscosity less than 5000 cps at 10 sec⁻¹ and a temperatureof at least 55° C., and effervescent agent. In one embodiment, theviscous component is solid at 23° C. In another embodiment, theeffervescent composition is a uniform, free-flowing granulation. In someembodiments, the effervescent composition includes from 5% by weight to30% by weight the viscous component, from about 5% by weight to about25% by weight of the viscous component, or even from about 10% by weightto about 20% by weight of the viscous component. In some embodiments,the effervescent composition includes a flow agent selected from thegroup consisting of silica, fumed silica, precipitated silica, magnesiumoxide, calcium phosphate, magnesium carbonate, calcium silicate, sodiumalumino silicate, and combinations thereof.

In some embodiments, an effervescent composition described herein is inthe form of a tablet. In one embodiment, the composition of the tabletfurther includes binder, lubricant, or a combination thereof. In anotherembodiment, the effervescent composition described herein is in the formof a free flowing powder. In another embodiments, an effervescentcomposition described herein includes an effervescent agent thatincludes citric acid and sodium bicarbonate, and further includessilica, lactose, magnesium stearate, and sorbitol.

In another aspect, the invention features a method of using aneffervescent composition described herein, the method including addingthe effervescent composition to an aqueous liquid.

The invention features a method of incorporating a viscous component inan effervescent composition. The effervescent composition provides aviscous component in a predetermined amount and in a convenient formthat is easy to handle.

The invention also features an effervescent composition that is capableof being tableted in an automated process and forming a tablet thatexhibits good structural integrity.

The effervescent composition can be formulated to readily disperse inaqueous-based compositions. The effervescent composition can beformulated to disperse the viscous component in water at a rate that isfaster relative to the rate of dispersion of the viscous componentalone.

Other features and advantages will be apparent from the followingdescription of the preferred embodiments and from the claims.

GLOSSARY

In reference to the invention, these terms have the meanings set forthbelow:

The term “effervescent composition” refers to a composition that evolvesa gas (e.g., carbon dioxide) when placed in an aqueous liquid.

The term “viscous component” refers to a component that is any one of asolid, semisolid and liquid at room temperature.

DETAILED DESCRIPTION

The effervescent composition includes a viscous component, and aneffervescent agent. The viscous component is a solid, semisolid or has aviscosity of at least 50,000 centipoise (cps), at least 100,000 cps, oreven at least 300,000 cps, at room temperature (i.e., from 68° F. to 77°F. (20° C. to 25° C.), and is a pourable liquid when heated to anelevated temperature. Preferably the viscous component exhibits aviscosity no greater than 5000 cps, or even no greater than 3000 cps ata temperature of at least 40° C., at least 55° C., or even at least 60°C., when measured at 10 second⁻¹ (reciprocal second), or even 1 sec⁻¹.

Suitable viscous components include Newtonian and non-Newtoniancompounds including, e.g., honey, molasses, wax, hop extract, kava, andmixtures thereof. A suitable hop extract is available under the tradedesignation YC Enhanced Oil hop extract from Yakima Chief, Inc.(Sunnyside, Wash.), one lot of which was found to have a viscosity of54,000 cps at 23° C. and 1 sec⁻¹ and 8,400 cps at 23° C. and 10 sec⁻¹and 2,900 at 40° C. and 1 sec⁻¹ and 700 cps at 40° C. and 10 sec⁻¹. Theviscous component is present in the effervescent composition in anamount suitable for its intended purpose. Useful formulations include aviscous component in an amount of at least 1% by weight, from about 5%by weight to about 30% by weight, from about 5% by weight to about 25%by weight, or even from about 10% by weight to about 20% by weight.

The effervescent agent preferably is at least one component of aneffervescent couple that includes an acid and a base. The effervescentcouple is activated when contacted with water, e.g., when the tablet isplaced in a glass of water. The water liberates the acid and base andenables the acid and base to react with each other to produce carbondioxide gas, which imparts carbonation to the aqueous composition. Atleast one component of the effervescent couple can also be an activeagent. Examples of useful acids include citric acid, ascorbic acid,malic acid, adipic acid, tartaric acid, fumaric, succinic acid, sodiumacid pyrophosphate, lactic acid, hexamic acid, and acid salts and acidanhydrides thereof, and mixtures thereof. Examples of useful acidanhydrides include citraconic anhydride, glucono-D-lactone, and succinicanhydride. Examples of useful acid salts include potassium bitartrate,acid citrate salts, sodium dihydrogen phosphate, disodium dihydrogenphosphate, sodium acid sulfite, and combinations thereof. Acid ispresent in the composition in an amount of from 5% by weight to about60% by weight, from about 5% by weight to about 30% by weight, or evenfrom about 10% by weight to about 20% by weight.

The base preferably is capable of generating carbon dioxide. Examples ofsuitable carbonate bases include sodium bicarbonate, sodium carbonate,sodium sesquicarbonate, potassium carbonate, potassium bicarbonate,calcium carbonate, magnesium carbonate, magnesium oxide, sodium glycinecarbonate, L-lysine carbonate, arginine carbonate, zinc carbonate, zincoxide and mixtures thereof. The base is present in the composition in anamount of from 10% by weight to about 60% by weight, from about 20% byweight to about 50% by weight, or even from about 30% by weight to about45% by weight.

The effervescent composition preferably includes a flow agent. The flowagent preferably enhances the ability of the effervescent composition toflow through the components of a manufacturing operation including,e.g., the components of an automated tableting operation (e.g., a hopperand a tablet press). Suitable flow agents include, e.g., silica (e.g.,fumed silica and precipitated silica), magnesium oxide, calciumphosphates (e.g., mono-, di- and tri-calcium phosphates), magnesiumcarbonate, calcium silicate, sodium alumino silicates, and combinationsthereof. A useful fumed silica is commercially available under the tradedesignation CAB-O-SIL from Cabot Corp. (Boston, Mass.). The flow agentis preferably present in the composition in an amount of at least 0.5%by weight, from about 3% by weight to about 20% by weight, or even fromabout 5% by weight to about 15% by weight.

The effervescent composition can be in a variety of forms including,e.g., powder (e.g., a free flowing granulation), tablet, capsule, andpellet. The effervescent composition can be prepared to exhibit adesired dissolution rate. Useful effervescent tablets includeeffervescent tablets having a hardness of at least 3 kiloponds (Kp), atleast 4 Kp, from about 5 Kp to about 15 Kp, or even from about 5 Kp toabout 10 Kp, as measured on a standard hardness tester fitted with astrain gauge. In one embodiment, the tablets are formulated to weighabout 5000 mg and preferably dissolve in excess boiling water in lessthan 300 seconds, less than 100 second, or even less than 60 seconds.

When in the form of a tablet or capsule, the composition preferablyincludes binder, lubricant, and combinations thereof. Examples ofsuitable binders include, e.g., starches, natural gums, cellulose gums,microcrystalline cellulose, methylcellulose, cellulose ethers, sodiumcarboxymethylcellulose, ethylcellulose, gelatin, dextrose, lactose,sucrose, sorbitol, mannitol, polyethylene glycol, polyvinylpyrrolidone,pectins, alginates, polyacrylamides, polyvinyloxoazolidone,polyvinylalcohols and mixtures thereof.

The effervescent composition includes a sufficient amount of binder toassist in holding the components of the composition together in the formof a tablet. Preferably binder is present in the composition in anamount of from 10% by weight to about 60% by weight, from about 15% byweight to about 50% by weight, or even from about 25% by weight to about40% by weight.

Various lubricants are suitable including water dispersible, watersoluble, water insoluble lubricants and combinations thereof. Preferredlubricants are water soluble. Examples of useful water solublelubricants include sodium benzoate, polyethylene glycol, L-leucine,adipic acid, and combinations thereof. The composition can also includewater insoluble lubricants including, e.g., stearates (e.g., magnesiumstearate, calcium stearate and zinc stearate), oils (e.g., mineral oil,hydrogenated and partially hydrogenated vegetable oils, and cotton seedoil) and combinations thereof. Other water insoluble lubricants include,e.g., animal fats, polyoxyethylene monostearate, talc, and combinationsthereof.

The effervescent composition preferably includes a sufficient amount oflubricant to enable the composition to be formed into tablets andreleased from a high speed automated tableting press in the form of atablet. The effervescent composition preferably includes water solublelubricant in an amount of from 0.1% by weight to about 15% by weight,from about 0.1% by weight to about 10% by weight, from about 0.5% byweight to about 5% by weight, or even from about 0.5% by weight to about3% by weight.

The effervescent composition can also include water insolublelubricants. Preferably effervescent composition includes less than 3% byweight water insoluble lubricants.

The effervescent composition can also include other ingredientsincluding, e.g., flavor agents, fillers, surfactants (e.g., polysorbate80 and sodium lauryl sulfate), color agents including, e.g., dyes andpigments, sweetening agents, and combinations thereof.

In preparing the effervescent composition at least some of thecomponents are preferably heated to a temperature of at least 40° C.,from 40° C. to 70° C., or even from 45° C. to 65° C., prior to beingcombined with one or more of the other components of the effervescentcomposition. In some embodiments, the viscous component is stirred(e.g., subjected to a shear stress) prior to combination with anothercomponent of the effervescent composition.

The effervescent composition is preferably stored in a moisture-proofpackage e.g., sealed foil containers (e.g., bags and pouches), sealedplastic bags, blister packs, desiccant capped tubes, and combinationsthereof. A number of tablets or capsules can be placed in a singlepackage.

The effervescent composition can be formulated for use in a variety ofapplications including, e.g., dispersing in an aqueous-based composition(e.g., water) at a variety of temperatures (e.g., refrigerated, roomtemperature, and boiling (e.g., boiling water)).

The invention will now be described by way of the following examples.

EXAMPLES Test Procedures

Test procedures used in the examples include the following.

Viscosity

The viscosity measurement is obtained using a Haake RS100 controlledstress rheometer (Haake). The rheometer is set up with a parallel platemeasuring system in which the bottom plate is fixed and the temperatureof the sample is controlled using a TC-81 Peltier temperaturecontroller. The upper plate is 35 mm diameter and is rotated at aprogrammed ramp from 0 sec⁻¹ to 50 sec⁻¹ shear rate and then from 50sec⁻¹ to 0 sec⁻¹ shear rate. The sample is tested by placing a from 2 to3 cubic centimeters of sample on the bottom plate and raising the bottomplate until the gap to the upper plate is 2 mm. The sample completelyfills the gap between the two plates and excess is carefully scrapedaway. The samples are equilibrated to the specified temperature beforethe measurement is obtained. A solvent trap apparatus is employed tominimize evaporation at higher temperatures. Viscosity values aredetermined during the ramp down from 50 sec⁻¹ to 0 sec⁻¹ at shear ratesof 1 sec⁻¹ and 10 sec⁻¹.

Example 1

The effervescent composition of Example 1, which included hops extracthaving a viscosity of 54,000 cps at 23° C. and 1 sec⁻¹ and 8,400 cps at23° C. and 10 sec⁻¹ and 2,900 at 40° C. and 1 sec⁻¹ and 700 cps at 40°C. and 10 sec⁻¹, was prepared as follows. Into a first container wasblended 29.7 kg anhydrous citric acid fine granular 50 USP/FCC, and 26.4kg instant sorbitol FGPh, and 2,200 g magnesium stearate. Into a secondcontainer was blended 37.4 kg sodium carbonate (Grade 50), 37.4 kgsodium carbonate (Grade 100), 7,700 g sodium bicarbonate No. 5, and 28.6kg FAST-FLO spray dried modified lactose monohydrate (#316 NF) ForemostFarms (Rothschild, Wis.). The first and second containers were placed inan oven, preheated to 50° C.+/−2° C., for at least 14 hours prior tofurther compounding.

The heated contents of the second container were added to a ribbonblender, which had been preheated to 50° C.+/−2° C. using belt heaters,followed by the addition of 15.4 kg CAB-O-SIL fumed silicon dioxide(Cabot Corp., Boston, Mass.), and then the contents of the firstcontainer. The components were blended for 30 minutes with the cover ofthe blender closed. Then 35.2 kg YC Enhanced Oil hop extract (YakimaChief, Inc., Sunnyside, Wash.), which had been warmed in a warmingvessel, was added slowly to the ribbon blender. The mixture was blendedfor from about 30 to 60 minutes.

The resulting composition was a uniform, free-flowing granulation thatdid not stick to the sides of the blender.

The effervescent composition was then transferred to a tablet presshaving a one inch tool to form tablets weighing from approximately 4.75g to 5.25 g. The tablets were pressed to a hardness of from 3 Kp to 9Kp.

The tablets had an average weight of 5.02 g, a thickness of 0.256 inch,and a hardness of 7.0 Kp.

Two tablets were then placed in 200 mL of boiling water and wereobserved to completely dissolve in 163 seconds.

Example 2

An effervescent composition including kava was prepared by adding 137.5g kava extract containing stevia (the kava had a viscosity of 14,000 cpsat 55° C. and 1 sec⁻¹ and 4,500 cps at 55° C. and 10 sec⁻¹), which hadbeen preheated to a temperature of 60° C., to a composition that hadbeen preheated to 60° C. and included 467.5 g sodium carbonate #100, 220g citric acid, 165.0 g FASTFLO spray dried modified lactose monohydrate(#316 NF) Foremost Farms (Rothschild, Wis.), 220 g sorbitol, 103.1 gCAB-O-SIL silicon dioxide (Cabot Corp., Boston, Mass.), 48.1 g sodiumbicarbonate #5, and 13.8 g magnesium stearate. The kava was added to themixture over a period of 90 seconds. The mixing and heating weremaintained for ten minutes. The composition was then cooled to roomtemperature. The composition was a uniform, free-flowing granulation.

The effervescent composition of Example 2 was then formed into tabletson a hand press. The tablets had a mass ranging from 5.05 g to 5.24 g, athickness of from 0.322 inch to 0.330 inch and a hardness of from 5.0 Kpto 5.5 Kp. The tablets, when placed in 200 mL of room temperature water,were observed to form a cloudy composition having a yellow residue after15 minutes.

Other embodiments are within the claims.

1. An effervescent composition comprising: from about 5% by weight to 25% by weight of a viscous component exhibiting a viscosity greater than 50,000 cps at 23° C. and a shear rate of 1 sec⁻¹ and a viscosity less than 5000 cps at a temperature of at least 38° C. and a shear rate of 1 sec⁻¹, and said viscous component is selected from the group consisting of hops extract, kava, molasses, honey, or a combination thereof; an effervescent agent comprising an acid and a base; and from about 3% by weight to about 20% by weight of a flow agent selected from the group consisting of silica, fumed silica, precipitated silica, magnesium oxide, calcium phosphate, magnesium carbonate, calcium silicate, sodium alumino silicate, or a combination thereof, and said effervescent composition is in the form of a uniform, free flowing granulation.
 2. The effervescent composition of claim 1, wherein said viscous component comprises hops extract.
 3. The effervescent composition of claim 2, comprising from about 10% by weight to about 20% by weight of the hops extract.
 4. The effervescent composition of claim 2 further comprising a binder, a lubricant, or a combination thereof.
 5. The effervescent composition of claim 1, wherein said flow agent comprises from about 3% by weight to about 20% by weight silica.
 6. The effervescent composition of claim 1, wherein said flow agent comprises from about 5% by weight to about 15% by weight silica.
 7. The effervescent composition of claim 2, wherein said effervescent agent comprises citric acid and sodium bicarbonate, and said effervescent composition further comprises: lactose; magnesium stearate; and sorbitol.
 8. A tablet comprising the effervescent composition of claim 2, said tablet having a hardness of at least 3 kiloponds and disintegrating in boiling water in less than 300 seconds.
 9. The tablet of claim 8 having a hardness of from about 5 kiloponds to about 15 kiloponds.
 10. An effervescent tablet comprising: from about 5% by weight to 25% by weight of a viscous component selected from the group consisting of hops extract, kava, molasses, honey, or a combination thereof; an effervescent agent comprising an acid and a base; and from about 3% by weight to about 20% by weight of a flow agent selected from the group consisting of silica, fumed silica, precipitated silica, calcium silicate, sodium alumino silicate, or a combination thereof, and said effervescent tablet comprises a uniform composition, has a hardness of from about 5 kiloponds to about 15 kiloponds, and disintegrates in boiling water in less than 300 seconds.
 11. The effervescent tablet of claim 10 further comprising at least one of a binder and a lubricant.
 12. The effervescent tablet of claim 10, wherein said effervescent agent comprises citric acid and at least one of sodium bicarbonate and potassium bicarbonate, and said effervescent tablet further comprises: lactose; magnesium stearate; and sorbitol. 